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American Mineralogist; March 2000; v. 85; no. 3-4; p. 449-465
© 2000 Mineralogical Society of America
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Spectroscopic and structural properties of synthetic micas on the annite-siderophyllite binary: Synthesis, crystal structure refinement, Mössbauer, and infrared spectroscopy

Günther J. Redhammer1,*, Anton Beran2, Julius Schneider3, Georg Amthauer4 and Werner Lottermoser4

1 Institute of Crystallography, Rheinisch-Westfälische Technische Hochschule Aachen, Jägerstrasse 17/19, D-52056 Aachen, Germany
2 Institute of Mineralogy and Crystallography, Geocenter, University of Vienna, Althanstrasse 14, A-1090 Vienna, Austria
3 Institute of Crystallography and Applied Mineralogy, University of Munich, Theresienstrasse 41, D-80333 Munich, Germany
4 Institute of Mineralogy, University of Salzburg, Hellbrunnerstrasse 34, A-5020 Salzburg, Austria

Correspondence: * E-mail: guenther.redhammer{at}sbg.ac.at

The effect of the incorporation of Al-Tschermak’s molecule to the trioctahedral potassium mica annite {K}[Fe3]<AlSi3>O10(OH)2 on local and average structure has been investigated by hydrothermal synthesis, structure refinement of X-ray powder diffraction data, Mössbauer and infrared spectroscopy. The various types of brackets indicate different structural sites. Samples with compositions {K}[Fe3–xAlx]<Al1+xSi3–x>O10(OH)2 were prepared by hydrothermal techniques. The maximum solubility of Al3+ is limited to x = 0.92 at 500 °C and to x = 0.82 at 700 °C. The main factor controlling the substitution limits is the ditrigonal distortion of the tetrahedral rings. Lattice parameters decrease linearly with increasing Al3+ content of the mica. A considerable decrease of M2-O and nearly no change of M1-O bond lengths with increasing Al3+ contents is indicative of preferred occupation of the M2 site by [Al3+]. Changes in K-O distances are also very pronounced and reflect the ditrigonal distortion of the tetrahedral sheet. The bimodal ferrous quadrupole splitting distribution (QSD) in annite, extracted from Mössbauer spectra, becomes narrower and more centered around 2.60 mm/s with increasing Al3+ contents, and its evolution suggests an increasing deviation from ideal octahedral coordination of Fe by O, illustrated by the increasing octahedral flattening angle {psi}. The population of individual QSD components proves that it is impossible to resolve cis and trans M-sites in micas by Mössbauer spectroscopy. In the hydroxyl stretching region, up to 7 bands are observed in the infrared spectra which correspond to OH groups adjacent to 3 Fe2+ (N-bands), to OH groups coordinated by Fe2+, Al3+, and Fe3+ (I-bands) and to configurations having one octahedral vacancy (V-bands). N- and I-type bands are shifted toward lower wavenumbers with increasing Al3+ content because of increasing OH···Otet interactions.




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